Automatic distillation testing



May 6, 1952 J. M. JONES ETAL AUTOMATIC DISTILLATION TESTING Filed June16, 1948 hv. M QNN vr MLN U21/145s 70 JST/P f NVENTORS M Jo N55 J0 EYTToENEz/s Patented May 6, 1952l UNITED STATES PATENT OFFICE AUTOMATICDISTILLAT-ION TESTING James M. Jones and John ,L llstranahan, PortArthur, Tex., assignors to The Texas Company, New York, N. Y., acorporation of Delaware Application J une 16, 1948, Serial No.\33,418

3 Claims.

In the industrial practice in the distilling arts it is commontoregulate the distillation by means of the distillation test of samplesobtained in the distilling operation. In ordinary practice a sample istaken from the equipment, sent to the laboratory where the distillationtest is made and the results then reported to the Stillman. There isnecessarily a considerable lapse f time between the time when the sampleis taken and when the Stillman is advised of the test and this lapse oftime obviously makes control of the distilling operation diiilcult sincethe actual conditions in the equipment when the Stillman is 'advised ofthe test may be considerably different from that obtaining when thesample was drawn. In accordance with vthe invention, provision is madevfor taking a sample and testing it in testing apparatus directlyconnected t0 the ldistilling equipment. By means of the invention thesample is subjected to distillation in the vtest apparatus and `alterthe distillation is completed, the heating of the test still isautomatically stopped and a fresh sample is withdrawn from thedistilling operation for the distillation test. In this way successivesamples may be expeditiously tested and the stillman is kept constantlyaware of the conditions in the distilling lequipment.

In accordance with the invention, the heating of the test still iscontinued beyond the point at which the end point of the sample isreached, a temperature is taken at a point in the -test still whichreflects the resultant increased temperature above the end pointtemperature and apredetermined temperature point in this highertemperature range `is utilized for automatically stopping the heating ofthe test chamber and admitting another sample for testing.

The invention` will be fully understood by reference to the accompanyingdrawing which is diagrammatic in character and which illustrates apreferred embodiment of the invention.

A testing retort I0 preferably constructed of metal is provided with avapor line I I extending to a suitable condenser (not shown). A sampling.v2 line I2gse-rves to Withdraw a sample of liquid which it is desiredto test and discharge it into the 4distillation chamber I0. The samplingline communicates with any suitable source of the liquid -to be tested,such as a distillate Vline through which a stream of distillate isrunning, aidistillate receiving drum or tank, a'bubble tower tra-y -orthe like. The introduction of liquid through the sampling line to thevessel Il) is controlled `by a valve I4 operated by la solenoid I5.

' It is preferable to provide in the sampling Vline an fenlarged4chamber VI6 constituting an accumulation chamber to Yassure that anample sample is vtaken each time the valve vis opened. It is alsoadvantageous to provide a restricted portion I3 in the'sampling linedirectly adjacent the vessel I0 for the purpose of preventing orreducing any gas-flashback when the relatively cool sample is introducedinto the vessel I0 heated from a previous distillation test. Thesampling line preferably enters vthe distillation vessel at an acuteangle, as shown in the drawing.

'Heatffor the distillation is supplied by a heating element II.The'heating'element is adapted to `beconnected in circuit with asuitable source of electricity through a double-pole, doublethrow relayI8. A 11G-volt A. C. i's well adapted as fthe source of electric power.

A thermocou'ple I9 is disposed to indicate the distillation 'test'temperatures and is normally positioned 'in the vapor space 'of thevessel Ill. The @thermocouple is in circuit with a device 20 whichconverts voltage to pen movement and controls the movement of a pen 2|on a rolling chart '2'2 in response to temperature changes in thedistilling Vessel. The chart is operated by a motor v23 which is adaptedYto be connected in circuit through the relay I8 with the source ofelectricity. In lieu of the rolling chart 22 a circular .rotating chartmay be employed.

A second thermocouple 24 is in contact with the wall of the vessel I0,being preferably positione'd at usome intermediate or lower pointof thevessel. It is in a continguous position to the Wall of the vessel so asto register to some degree at least the temperature of the wall andreflect the higher temperature of the vvessel above the endpointtemperature. The thermocouple 24 is preferably vin circuit with a device2`1 which converts voltage to pen movement and controls the movement ofapen 28 on the chart 22. Thus a continuous 'indication of thetemperatures taken by the thermocouples i9 and 24 is shown on the chartv2 2. The "therm'ocouples may be seligenerating or V.p'ro'i/'ided withan extraneous source of power. The thermocouple 24 is in circuit with anamplifying device 25 adapted, upon a given temperature rise, to close aswitch to apply power to a solenoid coil 26 of the relay I8. Thesolenoid coil 26 is energized only upon a predetermined rise intemperature of the thermocouple 24 and is de-energized upon a given dropin temperature.

The solenoid I5 which controls the valve I4 in the sampling line, isadapted to be connected in circuitI with the source supply ofelectricity upon the energizing of the solenoid 26 of the relay I8.

In operation, assuming a sample of distillate to be in the distillingvessel I with the valve I4 closed and with the relay contacts closingthe circuit to the heating element II and to the chart motor 23 (asshown on the drawing), heat is applied to the distillate with resultantvaporization. The vapors pass to the condenser wherein they arecondensed. The temperature taken by the thermocouple I9 and indicated onthe chart, rises as the distillation proceeds. The temperature continuesto rise until the last portion of the liquid is vaporized and themaximum temperature point or end point is reached, after which thetemperature as reflected by the thermocouple I6, immediately drops dueto the absence of vapor flowing through the vapor line. The applicationof heat is, however, continued beyond this point and the temperatureregistered by the thermocouple 24 continues to rise until thepredetermined point is reached when the solenoid 26 is energized whichfunctions to throw the double-pole, double-throw relay, breaking thecontacts in the heating and motor circuits so as to stop the applicationof heat by the heating element I1 and stop the motion of the chart 22.

The energizing of the solenoid 26 also serves to close the supplycircuit to the solenoid I5, the activation of which serves to open thevalve I4 and permit a sample of liquid to flow through the sampling lineto the distilling vessel I0. The influx of the relatively cool liquidinto the vessel I0 reduces the temperature of the metal wall which isreflected by the thermocouple 24. When the temperature registered by thethermocouple 24 has fallen a predetermined amount, the solenoid 26 isde-energized thus breaking the contacts in the circuit of the solenoidI5 and permitting the valve I4 to close. The contacts in the heating andmotor circuits are closed with the result that the heating of the vesselI0 is resumed andthe chart 22 is again placed in motion. Thedistillation of the fresh sample is thereupon conducted.

The temperature of the thermocouple 24 for actuating the relay to openthe heating circuit and to actuate the valve in the supply line isselected as any convenient temperature Well above any expectediiuctuations in the end point temperature and which may be quicklyreached upon the continued heating of the test still after the end pointis reached. Thus, for example, in testing samples having end pointsapproximating 380 F. an actuating temperature of 460 F. has been usedand in testing samples running about 475 F. end point an actuatingtemperature of about 520 F. was used.

The test still may be readily correlated with any standard distillationtest desired such, for example, as the ASTM distillation test.

Although a preferred embodiment of the invention has been describedherein, it will be 4 understood that various changes and modificationsmay be made therein, while securing to a greater or less extent some orall of the benefits of the invention, without departing from the spiritand scope thereof.

We claim:

1. The method of automatically making successive distillation tests ofliquid samples withdrawn from a distilling operation that comprisesconducting a sample from the distilling operation through a valvedsupply line to a distillation test still, electrically heating said teststill to effect vaporization of the liquid therein, measuring thedistillation test temperature with a temperature indicating means at agiven point, continuing the application of the heating after the endpoint of the liquid sample is reached, measuring the temperature of thetest still with another temperature indicating means 4positioned toreflect the increased temperature above said end point temperature dueto said continuance of the heating, upon a predetermined increase intemperature of the latter temperature indicating means and through theagency of such indicated increased temperature point automaticallyopening the heating circuit to stop the heating of the test still andopening the valve in the supply line permitting the introduction of asucceeding liquid sample to the test still with resultant coolingthereof and reduction in temperature of the latter temperatureindicating means, and upon a predetermined decrease in temperature ofsaid latter temperature indicating means and through the agency of suchindicated decreased temperature point automatically closing the valve inthe supply line and closing the heating circuit to resume the heating ofthe test still.

2. The method of automatically making successive distillation tests ofliquid samples withdrawn from a distilling operation that comprisesconducting a sample from the distilling operation through a valvedsupply line to a distillation test still, electrically heating said teststill to eect vaporization of the liquid therein, measuring thedistillation test temperature with a temperature indicating means at agiven point, continuing the application of the heating after the endpoint of the liquid sample is reached, measuring the temperature of thetest still with another temperature indicating means positioned toreiiect the increased temperature above said end point temperature dueto said continuance of the heating, at a predetermined increasedtemperature point of the latter temperature indicating meansautomatically actuating a relay to open the heating circuit and stop theheating of the test still and to open the valve in the supply linepermitting the introduction of a succeeding liquid sample to the teststill with resultant cooling thereof and reduction in temperature of thelatter temperature indicating means and at a predetermined reducedtemperature point of the latter temperature indicating meansautomatically actuating the relay to close the valve in the supply lineand close the heating circuit to resume heating of the test still.

3. Apparatus for automatically making successive distillation tests ofliquid samples that comprises a distillation test chamber, a samplingline for charging liquid samples to the distillation test chamber, avalve in the sampling line, a solenoid adapted to control said valve toopen and close it, a heating element in circuit with a source ofelectricity and adapted to heat the distillation test chamber,temperature indicating means disposed to indicate the distillation testtemperatures, another temperature indicating means disposed to reflectthe temperature of a point in the wall of the distillation test chamber,a relay including a solenoid adapted to be actuated at a predeterminedtemperature point of the latter temperature indicating means above thetemperature of the distillation end point to open the heating circuitand actuate the valve-controlling solenoid and to open the valve in thesampling line permitting liquid to flow into the distillation testchamber causing the temperature of the Wall of the distillation testchamber to drop and at a predetermined drop in the temperature of saidlatter temperature indicating means to close the heating circuit to heatthe distillation test chamber and to de-energize the valve-controllingsolenoid to close the valve in the sampling line.

JAMES M. JONES. JOHN J. STRANAHAN.

REFERENCES CITED UNITED STATES PATENTS Number Name Date 1,863,346 Mooreet a1 June 14, 1932 ,2,069,490 Fenske Feb. 2, 1937 2,081,601 Ridgway May25, 1937 `2,086,808 Kallan July 13, 1937 12,226,097 Happel et al. 1 Dec.24, 1940 `2,240,952 Hetzer 'May 6, 1941 2,350,006 Wolfner May 30, 19442,366,949 Woppman Jan. 9, 1945 FOREIGN PATENTS `Number Country Date728,957 France Mar. 2, 1931

